Making of activated carbon



.July2,1946. .-A M -THOMSEN 2,403,140

MAKING oF ACTIVATED CARBON W Filed Sept. 28, 1942 Man/and In Ziev IN VUV TOR.

Patented July 2, 1946 UNITED STATES 'PATENT ol-Flcs y MAKING' or ACTIVATED kCARBON Alfred M. Thomsen, San Francisco, Calif., assignor to Pacific vAcetate and Chemical Company, a corporation of California Application September 28, 1942, Serial No. 459,884 2 Claims. (Cl. 252-289) This invention dealsl in general with the means whereby an acceptable type of activated carbon can .be produced from many types of material not otherwise considered suitable and, in addition with means whereby the cost of producing said charcoal can be greatly reduced. I

The process, in its entirety, is best understood by following the various steps indicated upon the attached ow sheet, but prior to the complete elucidation of same, 'some explanatory words, and

comparisons with existing methods, are appro.

In general it is held that the characteristics of an activated carbon are determined by its physical structure. The actual, phenomenon is still obscure. It is presumably due to the adsorption of the innite number of tiny pores acting upon suitable substances, generally such as have a rather heavy molecular structure. y l

It may be well to .consider what takes place when wood or woody substances are carbonized.A

In the breaking down of the carbohydrates of which wood is chiefly composed by 'the action of heat the carbon of same is principally left as a residue but a part is driven olf in volatile, compound form.

The primary carbon thusA produced vis presumed to be actually in some highly activated form and thus capable of absorbing apart of the pri-` mary tar simultaneously-produced. Such adl sorbed tar becomes carbonized, in` situ. and becomes a part of the residue left within the retort, a really very complex substance containing a hydrocarbon component, to which the generic name of charcoal is' applied;-l l The lobject of activation is to remove this Venvelope of tar-coke'from the charcoal and thus free the infinite number of tiny pores that have become choked with the tar residuum. Porosity is, of course, -`a very relative term. All charcoal is very porous and contains a great number of large pores, some large enough to be seen with the naked eye. But itis the infinite number of microscopic pores that only the mostvpowerful ofmicroscopes will detect that are the real active media.' 4

The apparently solid walls of the porous It has already been said that to free all these tiny pores of 4encrusting substances is the object of activation. It is accomplished by exposing the charcoal to agents that arecapable of removing saidincrustations. but all such are also to some extent capable of attacking the primary charcoal, whether it be formed from the original decomposition of carbohydrates or from the adsorbed tarry matter that subsequently are coked. It is` the object, therefore, to sov regulate matters that the minimum of desirable charcoal is removed in the process of activation.

Density of charcoal .is thus to some extent an .indication of the presence of a relatively large vHowever; it becomes possible to close up such 1 dense charcoall can be charcoalV consist entirely of this porous structure.r

coals seem to the naked eye tohave a glossy luster and a smooth surface on a fresh fracture. But

after activation this same charcoal will under a DOwerful microscope have a 'dead-black appear-.

ance entirely devoid of lustre.

large pores to .a considerable extent by impregvnating such low-density materials with a soluble carbohydratel or hydrocarbon. or both, and then carbonizing once more. In this manner a, very produced from even porous woods.

This method can also be applied to material which has been partially activated previously, and finely powdered activated char' can likewise be commingled with a binder. briquetted and re; distilled in which case a very dense charcoal extremely suited for activation can be produced.

' The principal agent used in activation is doubtless steam, which at temperatures permitting the Water gas reaction'has a selective action forthe complex encrusting matter leaving the residualI carbon in a highly activated form. However` even air alone or in the presence of steam also has its uses. The halogens at elevated temperatures have. a similar selective action and at lowe'r temperatures so has ammonia.

In any event,V a gaseous medium is contacted with the char to be activated at elevated temperatures, as high as 2400 F. being not uncommon. It follows that the heat required to raise relatively large amounts of gas to such temperatures isl considerable, and how to effect the raise is even more important as the transfer'of heatat such. temperatures is accompanied by' much technical difiiculty.

phase of the matter advantage is taken in one To overcome this method of'electric heating, the carbon itself. being the resistor. Such means are necessarily quite costly both in ilrst costaud in operation.

^ `For this reason all highly activated chars are decidedly costly and mitigate a great deal against their extended use in industry apart from where they must be employed.

be activated, said charcoal being contained in an insulated chamber, and activation will duly proceed.

The issuing gases will still retain almost all of theirsensible heat upon leaving the charcoal so they may evidently be passed through another brick checker and thus be stripped of their heat before they are discarded. Fresh activating gas may now be heated nearly to reaction temperature by passing through this checker and may then be raised to the required initial by passage through a supplementary heater which will. have very little work to do. The process thus becomes heat-recuperative and the design is' greatly simplified and cheapened.

This combination of relatively inexpensive plant and heat economy results in'low costs for activation. Almost any type of wood waste can be employed to make the charcoal and singularly suited as the medium for increasing the density of the char, or for briquetting, is that -form of wood in solution which we designate as the spent or waste liquors of the pulp industry.

The flow sheet shows as a preferred version such an operation in which wood or the like is carbonized to yield a char and the conventional gaseous products. These are scrubbed with a solution of `sodium carbonate, or other alkaline soda salt, thus salvaging the acetic acid produced as well as the condensed tar. Such recovery of sodium acetate is a help in reducing the cost and the. tar may be employed as indicated to increase the density of the char formed in tue of the weight of the additive carbon which has been deposited within its pores.

Activation'is thenext step. By means of the dotted lines I have indicated the duplex nature of such items as heat recuperators and the supplementary heating stoves. The solid line is used to indicate the normal flow, and the dotted line to indicate the corresponding action when the device is not .on stream." It will be evident that all such devices must be built in parallel, so that by reversal of ilow the heated device may give oi its heat to the gases it is desired to heat.

It will also be apparent that no claim is 'made for any originality in the chemical aspects of activation. Be the uid, air, or steam or any gas, or any combination of gases, it is apparent that the heat-recuperative cycle will function equally well. It is independent of the medium employed, hence on the flow sheet lit is simply lreferred to -as the activating gas."

- briquetting added to.said impregnation and then be re-activa-ted. Such powdered char may be only fresh charcoal or it may be a discard of fully activated material which is returned to the ycircuit in order that it may issue in a more desirable physicall condition.

Such minor modifications, or rather diverse applications, of the basal theme I consider as forming a part of this disclosure. Having thus fully described my process,

I claim:

1. The method of increasing -the density of a char which comprises; impregnating saidchar with a liquid medium which on distillation will yield a carbonaceous residue; facilitating said impregnation by inducing a partial vacuum in the primary carbonization of woody substances. l

In place of tar for this impregnation, or together with said tar, use may be made of soluble carbohydrates. Solutions of sugars and particularly of spent cooking liquor is here recommended. Impregnation will be aided if a partial vacuum is rst induced in thepores of the charcoal which then will readily become penetrated by the liquid medium.

A secondcarbonization is now resorted to, and the ilow sheet ,shows the resultant volatiles condensed while the' char has become denser by virthe pores of said char during said impregnation; submitting said impregnated charcoal to sumcient heat to drive oil the volatile portions of the impregnating medium, thus leaving the larger pores of the primary char partially filled with a secondary char.

2. The method of increasing the density "of a4 char setforth in claim 1, with the added vstep that said impregnation and said heating be repeated until the char has reached the pre-determined density. v

- ALFRED M. THOMSEN. 

